DE1469427A1 - Process for imparting a molecular orientation to threads made of a polymeric polyester - Google Patents

Description

German I. WIIGAND

MONKS

DIFL.-1NG. W. NIIMANN

HAMiUlO PATINTANWXLTf

N 15, 5TH NUSSIAUMSTIASSEIO TELEPHONES $ 5 54? *; $ -.

W.

Monsanto Company
St. Louis, Missouri (V.St.A.)

Procedure for granting a molecular orien4? I- »*». W. on threads made of a polymer polyester

The invention relates to an improved Terf a & ren for the production of objects from synthetic, high molecular weight linear polyesters · In particular the invention relates to an improved method to improve the surface properties of synthetic materials j items made from linear polyesters

The application of finishing or finishing agents on textile materials in order to impart certain desired properties to the textile goods or materials, e.g.

- 2. - - ■ "

Antistatic protection, stiffness, sizing, softness, slidability, water repellency, shrinkage resistance, flame-retarding properties or flame-resistance or the like the polyamides, foly esters, polyalkylenes, polyurethanes, polycarbonates, acrylonitrile polymers or the like. _{It is} known that the yarn tear strength can be increased significantly by using the drawing work processes, which include drawing the yarn threads after they have been formed in order to increase the molecular orientation. ... .. - .. -. -.-.- .. _; ■ ·. ... - ... ....'-: ■ .., -, ■ ..

Although the stretching process by various means can be carried out ι be with a brewery Yer * · drive two! thread feed devices used which commonly known as a feed roller and a draw roller are. A thread stretching is achieved by doing this Running rollers at different speeds,. the extent of stretching or tension being determined by the ratio of the peripheral speeds of the two rollers. . In order to locate the place or point at which the stretching takes place, a braking device is sometimes used placed between the feed roller and the stretch roller · In general, the braking device consists of

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a pin, the so-called "" drawing pin ", is about which the G _rn repeatedly wrapped * The draw pin results in the moving filaments frictional resistance brought about, whereby the occurrence of a stretching wird- caused in the area of the drafting pen" · The introduction of a frictional resistance to the local definition of the stretch is applied in those cases where a .Neigung to occurrence of uneven stretching is present, as by the application of this procedure, greater uniformity can be obtained _o. '. . ..

It was known that the drawing process can sometimes be easier if the yarn temperature during the Stretching is increased * Heating can be increased by onset a hot pen, a hot plate, or a hot Medium bath between the feed roller and the stretching or Draw roller of the stretching device or by using a heated feed roller o Elevated temperatures are effective because intermolecular forces result from the Increase in molecular activity will be decreased and accordingly the ratio of force required to stretch of the yarn to the force required to break it o Permissible temperatures which can be used for hot stretching change something to do with the type of polymer from which the yarn is formed, since the maximum temperature is used

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can be limited by the "softening" point of the polymer. It is common practice to use a hot stretch procedure when yarn for use in products that require high tensile strength, such as "B _o in manufacture of reinforcement cards (reinforcement cards) for inflatable tires

A particularly troublesome problem associated with de »·: connected routes at both room temperature and at elevated temperatures, the occurrence of yarn breakage during drawing ₀ Thus, one or more individual threads sometimes break in the yarn strand and beautiful wrap around the drawing roller or, which sometimes happens, the whole strand of thread may break, with production being interrupted until an adjustment can be made. Such a thread breakage not only affects labor and productivity, but also adversely affects product quality

The main cause of thread breakage during stretching is the creation of excessive tension on the yarn, which in turn are mainly due to frictional forces between the threads and the creation of excessive friction, when the yarn runs over the draw pin j if such a device is used, it is reinforced »

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It is; It is known that excessive yarn chipping resulting from the development of unacceptably high and variable frictional forces during drawing can be reduced by applying various anti-friction conditioning agents to the yarn before it is drawn. These agents are generally made from an aqueous one These factors are of considerable importance and cannot be used, for example _, if one is used -aqueous solvents are not regulated as a carrier.

It is known "that lasers or threads made from synthetic linear polyesters of high molecular weight, freshly spun, can be slowly cold drawn by hand or can be quickly hot drawn over heated surfaces according to the procedures described above" If, however, undrawn polyester fibers or - threads are allowed to age or are left to have a weakening effect ("lay ¹¹ ), the polyester fiber or the polyester thread changes. 4a, as is known, its amorphous

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fetur and the older thread or the aged fiber crystallizes, what stirs it? _f can dab the fiber or yarn material is highly fragile and difficult gleierhf Ormig stretch "This condition or this state is _s where the individual threads are on the draw pin during the drawing stage and. by winding the thread, "softens on & en stretching rollers, as discussed in the table below, accumulate or pile _f reinforced". In some cases, slow stretching can be applied geschwdndigkeiten "to facilitate this condition to assist in .gewissem extent, but this does much can be stretched in a given time period, the yarn or fiber or" Fadenmeoge _t tre & eiw limited "Although the Keigung ztt Erüchigkeit "iibermäßi-, called yarn tensions od" like _e, which, during the stretching of •. Leave it to older people or to a brook effective. Fibers or threads can develop * something by treating with yor; BestiEHtt.ten ^v known conditioning agents got, kind can be lowered »ordered a permanent ^ allowed to treatment masses _t which these with greater effectiveness

; Can solve difficulty.

One purpose of the invention is the Yerbesserong of the Yerf stage of stretching synthetic linear polyesters of high molecular weight »■ '"' ■ ■ '

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Another purpose of the invention is to provide static protection and lubrication or sliding action for improved treatment or processing of synthetic linear polyester threads of high Molecular weight «

Another purpose of the invention is to provide a method for reducing the tendency to "formation of vapors or fuming" ( "fuming") of equipment or M finishes on threads of synthetic linear polyesters of high molecular weight during hot stretching step "

Other purposes and advantages of the invention will be apparent from the description below

It has been found that the brittleness of yarns made from synthetic linear high molecular weight polyesters ₅ which are not fully stretched and the build-up of excessive yarn tension during stretching of the yarns can be substantially minimized by adding J before the stretching stage ™

they / treated with an aqueous emulsion, the solids content of which is about 70 to 100% by weight of a phosphate ester surface treatment agent and about 0 to 50% by weight of a mixture comprised of amine salts of various alkyl phosphates " It has also been found that this method not only facilitates the stretching process, but also makes it considerably easier Benefits given to the final yarn product, "

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For example, a sizing or finishing composition as described above has been found to provide improved stretch properties and stability to ticks in a high molecular weight synthetic linear polyester yarn after a lag time of 30 days retains _o

The phosphate ester surface treatment agents, which for the preparation of the aqueous emulsions according to the invention apply consist of compounds of the general formula

£ ~ B. - 0 - (CH ₂ CH ₂ O) _7 ₂ - p'afcO '

OM

in which R is an alkyl radical with 8 to 20 carbon atoms or an alkylphenyl radical in which the alkyl group has 8 to 20 carbon atoms, M is a hydrogen atom, an ammonium group or ea.es is an alkyl or alkaline earth metal, _s preferably potassium or sodium and η is an integer of 2 to 20, preferably 7 to 10, and from compounds of the general formula

- 0 - (CH ₂ CH ₂ O) _n -7- P = O

OM

in which R, M and ö have the meaning given above » Examples of phosphate ester surface treatment agents, which can be used for the purposes according to the invention are the sodium salt of the phosphate diester

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of oleyl alcohol reacted with 7 mol Äthjlenoicyd, the potassium salt of the phosphate diesel of oleyl alcohol reacted with 8 mol lithylene, diesel compounds are produced by mixing the corresponding alcohol with the ethylene oxide in the presence of a catalyst, ζ «B ₀ a trace of Sodium, and then adding phosphorus pentoxide _o

The JL ^ amine salts of Älkylphospha.ten used in the process according to the invention consist of alkyl phosphates of the general formula

(HO) _x - P - / "0 (MZ) H_7 _y

in which χ is an integer of 1 or 2, y is the difference or difference between 3 and x, R is a normal alkyl radical with 8 to 16 carbon atoms and KX is an oxyalkylenamine, which is made from a mono-, di- or triethanolamine, the ethanol derivative of monomethy1 - or dimethylamine or morpholine may consist represent _o optimum results can be obtained by g nit v / ground if mixtures are amine salts of alkyl phosphates for use different ,, the performance of Alkylphosphatmischung. increases as the proportion of the diester in the mixture rises to 50%. In general, the various alkyl phosphates are the reaction product of phosphorus pentoxide, a straight chain, saturated, primary monohydric alcohol having more than 6 carbon atoms and an oxyalkyleneamine, as described above.

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The practical. -Durchführung.des method Trema ß of the invention eligible synthetic linear condensation polyesters are those, which are formed from dicarboxylic acids and glycols, and mixed poly; esters, and modified polyesters and copolyesters "In highly polymerized condition, these polyesters and copolyesters can be formed into threads ododgl" or shaped -Will _o.

Particularly useful polyesters and mixed polyester-ge -.- ^J measure of the invention are those which on heating, ginem Glyko'len or more of the series HO (CH ^) ₁₁ QH in which H is an _integer 2-10 means, with one or more dicarboxylic acids or the ester-forming derivatives thereof ^ are obtained. Invention ge / hö-ren Tei? Ev "lithaläure, isophthalic acid, oebacinsKuial, Adip jr ^ s Βλίτ e _s , Pr Carboxypheno, acetic acid, succinic acid, ^, pZ-Dicarboxybiphenpl, ρ, ρ ¹ -Dicarboxycarbanilid, pjarboxyth'-Docarbanilid, pjarboxyth'-D , p ^T - · _v dicarboxydipiienylsulfon, p-carboxyphenoxyacetic acid, ■ p-carboxyphenoxypropionic acid, p-carboxyphenoxybutyric acid, p-> carboxyphenoxyvaleric acid, p-carboxyphenoxyhexanoic acid,. ■■ - .. pP-dicarboxydiphenylethane, ρ _t p'-diearboxydiphenylpropane, P, p -diearboxydiphenylbutane, ρ, ρ'-diearboxydiphenylpentane, ρ, pi-dicarboxydiphenylhexane, ρ, ρ

909804/1239 bad or, g _IN al

ρ, p '-Dicarboxydi riieny loctan, ρ, ρ' -Dicarboxydiphenoxyathan, ρ, ρ '-Dicarboxydi ^ iienoxypropan, ρ, ρ' -Dicarboxy diphenoxybutane, ρ, ρ'-dicarboxydiphenoxy / äpentaran, ρ, ρ'ydi :> Lienoxyhexane, 3-Al] Qr 1-4— (β-carboxyethoxy) -benzoic acid, oxalic acid, -glutaric acid, pimelic acid, suberic acid, azelaic acid and the dioxy acids of ethylene dioxide of the general formula HOOG - (OH ₂ ) _n - 0 - OH ₂ OH ₂ - O- (0H ₂ ) _n - OOOH

in which η denotes an integer from 1 to 4, and the ^ aliphatic and oycld.aliph.at aryl esters and half esters, ammonium salts and amine salts and the acid halides of the compounds listed above, examples of glycols which are used in the practical implementation of the process According to the invention, ethylene glycol, trimethylene glycol, tetramethylene glycol, decamethylene glycol, ododglo polypropylene terephthalate is preferred, however, due to the immediate availability or availability of terephthalic acid and ethylene glycol from which it is made in proportion high melting f puÜkt of about 2 ^ 0 ° - 255 ° O, this property especially in the manufacture of threads in the textile industry. desired is _o

To the modified polyesters and mixed polyesters ^ which can be used in the practice of the method according to the invention include those polyesters,

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as stated above, those with dialkylometers of saturated, essentially linear aliphatic dicarboxylic acids with a content of 20 carbon atoms of the general formula

S i ° n ^H 2n ₊ A 8

C - 0 -

are modified, in which R and R _{0 are} alkyl radicals with 1 to ^ 10 carbon atoms and preferably alkyl hydrocarbon radicals with 1 to 5 carbon atoms, including methyl, ethyl, propyl, isopropyl, n-butyl, sec-butyl, Isobutyl, n-amyl, isoamyl radical ad · dgl «, A is a linear, saturated, aliphatic radical with 14 to 18 carbon atoms in its chain, η is an integer from 1 or 2 and y is an integer from 0 to 2« the total number of carbon atoms in A and the side chains thereof is 18 »R, - and Rp can be the same or different alkyl radicals · examples of Bialkylestern extending fcemäß the invention proved braucti- w bar, dialkyl comprise 1 to 1.20-eicoeandioat , Dialky 1τ-8-äthyloctadecan-1,18-dioat, DialkyIdimethyloctadecan-1,18-dioat, DialkyIdimthylnertdican-I, 16-dioat or the like ·, whereby the dialkyl groups are methyl, ethyl, propyl and similar .. groups mean, including alkyl hydrocarbon radicals having 1 to 5 carbon atoms en. Mixtures of any of the materials noted above can be used. Examples include mixtures

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approximately
from “fee” 20 to 80% by weight of dimethyl-1,20-eicosandioate and about 80 to 20% by weight of dimethyl-S-ethyloctadecane-18-dioate are completely usable a molar basis usually a molar equivalent of a Mi .chung from · two urten of üialkylestern of aromatic and OPQ Dicarbons3uren and a molciren excess glycol dec _o in the mixture of dialkyl esters are the aromatic dicarboxylic Dial a ky in! "-! close of about 65 to 95% by weight; i- and the dialkyl esters of the aliphatic G ^ Q -dic acids present in amounts of about 35% to 5%

Among the modified polyesters and Miscxipolyjaiestern which of the invention are useful in accordance with the practice of the method, are the polyesters and copolyesters, as indicated above, which are modified with chain-terminating groups having hydrophilic properties, zobo the mono-functional, esterbildenden polyesters * of the general formula

RO- Z "(CH ₂ ) _m O_7 _x (0H ₂ ) _n - OH

in which R is an alkyl group with 1 to 18 carbon atoms or any aryl group with # to 10 carbon atoms, m and η are integers from 2 to 22 and χ is an integer indicating the degree of polymerization, i.e. L χ is an integer Number from 1 to 100 or above, represent »Examples of such compounds are methoxypolyethylene glycol, ethoxy

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polyethylene glycol, η-ϊ-ropoxypolyäthylenglykol, Isopropoxypo-Iyäthylenglykol, Butoxypolyäthylenglykol, Phenoxypolyäthylenglykol, methoxypolypropylene glycol, metho ^ ypοIybutylenglykol, phenoxypolypropylene glycol, Phenoxypolybutylenglykol, Methoxypolymet jylenglykol od _"0 Suitable like PoIyalkylvinylather with a terminal hydroxyl group are risate the Additionspolyme- represented by the iiomopolymerisation of alkyl vinyl ether ',' in which the alkyl group contains up to Λ 4 carbon atoms, are prepared _o Seisr.iele such feiettenbeendigungsDiittel are hydroxy polymethylviny lather, pol Hydroxypolyäthylvinyläther, Hydroxypolypropylvinyläther, hydroxy, - '^ but3 1vin5 ^r LAETHER, Hydroxypol3 / isobut; / lvinyläther ou , d "dgl _o The chain-terminating agents or compounds can be used in the production of the modified polyethers in Kengen in the range from 0.05 mol used in the cocktail mix will be used. It should be noted that when chain-terminating agents are used alone, that is _, without a chain-branching agent, the maximum amount which can be used in the action is 1.0 mol controlled amounts of chain branching agents together with the chain terminating agents, the introduction of an increased amount of the latter into the polymer chain than is otherwise possible when using the chain terminating agent alone »·

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It can be easily seen that the weight percentage Amount of chain terminating agent, which according to the invention can be used as the molecular weight of the agent changes. The range of mean molecular weight, the chain dressing agents, which are to be used according to the Invention are suitable "is from 500 to 5000, where such Agents with a molecular weight in the range from 100 to 3500 are preferred

Materials which are suitable as chain branching agents or chain crosslinking agents and which are used for enhancement the viscosity or the molecular weight of the polyester are used, are polyols with a higher functionality than 2, doh * they contain more than 2 functional groups, for example hydroxyl. Examples of suitable compounds are pentaerythritol, compounds of the general formula

R -, (0H) _n

in which R is an alkylene group with 3 to 6 carbon f atoms and η is an integer from 3 to 6, e.g. glycerol, sorbitol, hexanetriol-1,2,6 or the like, compounds the general formula

R-

in which R is an alkyl group with 2 to 6 carbon atoms means, for example, Tri »ethylolätk * n, Triaethylolpiopan and

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Similar compounds to TrimethyloHiexan and the compounds the general formula

in -which η means an integer from 1 to 6 * Examples for compounds of the above formula are trimethylolbenzene-1,3,5τ Triethylolbenzene-1 »3.5 j od similar *

Aromatic polyfunctional acid esters can according to of the invention can also be used as chain branching agents, in particular those of the general types formula

in which E, E ¹ and E "represent alkyl groups with 1 to 3 carbon atoms and E" ¹ hydrogen or an alkyl group with 1 to 2 carbon atoms. Examples of compounds of the above formula are trimethyltrimesate, tetramethylpyromellitate, tetramethylmellophonate, trimethylhemimellitate, trimethyltrimellitate, tetramethylprehnitate In addition, mixtures of the above esters, soft in the

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I ^ 0 3 <♦ / L f

fr

- 17- "

practical synthesis can be used "" Doho that in most cases when any compound of the above formula is prepared, other related compounds of the same "formula ¹ i &'are present in small amounts as impurities." This, however, affects the " Compound as a chain branching agent in the production of the modified s. Polyester and mixed polyester, as described here, niclrb ,, ....... . ' Λ

Me. KettenyerzweigungSr or crosslinking agents can be used in the production of polyester and mixed polyesters in amounts .im 3ereiC ^ νρη 0,, O ^ Μο.1-9έ to 2.4 mol%, based on the amount of Diearbonss.ure or derbster which are reached in the Eeaktionsmischung to the application that uses <> the preferred range of Kettöntoerzweigungsmittel for use according to the invention is between "0", 4 timcL · Ί, Θ ¹ mol%. " In the practice Ausfohrung the method of the invention, the berechneten.Mengen- of Zettenbeendigungsmittel or Eettenbeendigungsmittel and Kettenverzwei- or crosslinking agent ^r "iii äktioiisgefäß the R 'zti Be ^ - ·

The first stage of the esterification reaction was introduced and the reaction proceeds as with "- 'any iea? bökä'nttten Mineralization polymerisationo ^. . ·

. The highly polymeric, linear condensation polymers of polyesters or pol; $ jlmiden, which in the molecular Structure of a substantial proportion of repetitive

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Gr up .en of the following structural formula

- O -OH ₀ "- HC ^ GH - GE ₀ - O '"

^X 2

have, wherein the cyclohexane ring in the cis or trans isomers may be made thereof, the method of the invention for the arrival _Ä can reach "These polymeric linear polyesters and polyesteramides can be produced according to a method in which one phrase in the practice of ( 1) either the cis or the trans isomer or a mixture of these isomers of 1,4-cyclohexanedimethanol alone or mixed with other bifunctional reactants with (2) a bifunctional carboxy compound "condenses ο ■" - "■"--.-'-"-■" ■ ■■ "· ' ■

The bifunctional reactants, which. . · can be used do not contain any other reactive substituents which could lead to the formation of a highly poly- " meren, linear polymer, if they are with 1,4 ~ cyclohexanedimethanol or a mixture thereof with such bifunctional ones Heat participants are condensed, disturb The for the production of linear - ^ ondens ^ atiünspolymerisaten suitable bifunctional reaction participants are pretty much.

well known and discussed earlier

"J - ·, ..., - D, as. b | i any of the processes for the preparation of Konöensationspolymerisaten used Λ , 4-Cyclohexanedimethanol in combination with a further

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dual reactants are used; "for example ie * -ee when using a mixture of glycoles * (Es is advantageous, the 1, 4-Oyclohexanedimethanol in Amounts which are at least equal to 50 mole percent of the total

~ fri-V S _v · V * · ί. <· -. * ■. · TLA · «.-.

such mixed reactants used are / f although smaller proportions can also be used ») The various bifutectional misire reaction participants, which is used in mixture with 1,4-cyclohexanedimethanol ^ include other glycols and compounds which do not necessarily react with a glycol, e.g. a «- * ·» Amino alcohol ο Such miBchreaktanten (eoreactants) include diamines or aaaijiocarboxy compounds.

The functional group-containing bifunctional Eeaktionsteilnehmer which _f with 1,4-cyclohexanedimethanol or mixtures thereof may be condensed therefrom, are bifunctional compounds which can be condensed to form high polymers, linear Kondensationspolymerisaten, etc. Such Sifunktionelle compounds can only inter-reactive with a G-lykol or they can be both (a) mixed-reactive in the sense that they can be used instead of or as a partial replacement for the glycol in a polyester, and also [^) interreactive in be in the sense that they are with a glycol or a bifunctional compound, which instead

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of glycol can be used .. condense ,. For example, δ-aminocaiic acid is both mixed-reactive in that the amino group is of the type which can be used in place of a hydroxy radical of a glycol, and also interreactive in the sense that the carboxyl group with the hydroxyl group of a glycol or the amine of a bifunctional compound, which instead of a glycol can be used reacts _β bifunctional compounds which are merely interreaktionsfäaig with a glycol, include dicarboxylic acids include carbonates ododgl · The other bifunctional compounds interraktionsfähigen amino or carboxy Hydroxycarboxyverbindungen _o

Those used in the method according to the invention

specific

modified linear condensation polyester own feeeeasche
ekeee viscosities in the range from about 0.1 to 1.0, these being fiber- and thread-forming polymers »The term" specific viscosity "used here is represented by the formula ·

reproduced, where

Flow time of the polymer solution in seconds

relo flow time of the solvent in seconds The viscosity of the polymer solutions and the solvent are determined in such a way that the solutions are determined

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and allows the solvent to flow under the action of gravity at 25 ⁰ G through a capillary tube · In all determinations of polymer solution viscosities, a polymer solution containing 0.5% by weight of polymer dissolved in a solvent mixture of two parts by weight of phenol was used and one part by weight of 2,4,6-trichlorophenols and 0.5% by weight of water, based on the total weight of the mixture

The aqueous emulsions which can be used in practicing the process according to the invention can contain up to 20% solids by weight without exceeding the viscosity limits normally used for conditioning agents which are used in yarn preparation, being about 2 to 15% solids are generally preferred. The term "solids" used here means the totality of the constituents excluding the aqueous vehicle, regardless of the physical state. The solids can be about 70% to 100% by weight. of the phosphate ester surface treatment agent, as described above, and about 0 to % of the amine salts of various alkyl phosphates, as indicated above, contain ·

When making the composition or batch Conventional procedures can be applied to the aqueous emulsion. In accordance with a simple and

In a convenient way of working, the materials are simply mixed together, heated until the solid materials melt, 909804/1239 ^ _omiml

and then the molten mixture of constituents to the aqueous carrier with vigorous mechanical stirring to egeten ^ »£ During this Zugabestuf the water" are held at an elevated temperature, which "lies at or above the melting point of the components ₀

In general, both cold stretch and Hot stretching operations get good results if the Conditioning agent is applied in such an amount that the solids deposited on the laser or the thread about 0.1 to 1.5% "based on the weight of the fiber or thread ^ result". Although lesser or greater amounts are used optimum results are obtained when the amount of solids deposited on the fiber or thread was within this range

As has been established, as described above Treatment agents are applied to the filaments or fibers immediately during or after spinning and before drawing. brought line customary and expedient method of application consists in that one the fibers or threads in contact with a roller with the treatment agent during their movement or their advancement in the course of production brings, which is circulated so that its lower part is immersed in a trough containing the treatment agent ο The treatment agent is from a. Storage container pumped to the trough or other container, a constant by means of an overflow pipe or similar device Mirror is maintained »Other suitable work-

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Ways and facilities can be applied, e.g. Use a wick or a split roll or the fiber can be e: m containing the treatment agent Bad to be aged.

The fibers or threads described above can be modified by incorporating various modifying agents. Examples of suitable modifying agents which can be incorporated into the fibers or threads are pigments, plasticizers, resins, diluents, water-repellent substances, waxes, gloss modifiers üierungsmittel, flame retardants or flame-proofing agents, anti-static agents, plasticizers od * like _e

The invention is illustrated below by way of examples explained in more detail in which both the advantages that arise in terms of improving the stretching process as can also be shown in the yarn products finally obtained «|

example Λ

Filaments were melt extruded or - ejected one at about 6% based on the weight of the polyethylene - terephthalate, methoxy polyethylene glycol with a molecular weight of about 2000 and about 0.125% »based on the weight of the polyethylene terephthalafe, modified by pentaerythritol Polyethylene terephthalate polymer produced on no finishing or finishing was applied to these threads

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The threads were then lagged or kept for 17 hours at room temperature, about 2J ⁰ G., after which time they could not be uniformly cold or hot drawn. Further threads were kept at room temperature for 8 days, at which point they were neither cold or hot stretched; they were so brittle that at a stretching amount or ratio of 5 »2 there was no ^ contiguous or

ι. ".Ui

Wf continuous stretching force could be maintained for a short period of 5 minutes

Example 2

By means of melt extrusion or ejection of a Polyäthylenterelithalatpolymerisats, whichjp. with about 6%, based on the weight of the polyethylene terephthalate, of methoxypolyethylene glycol with a molecular weight of about 2000 and about 0.125 % based on the weight of polyethylene terphthalate, modified by pentaerythritol, threads were produced an aqueous emulsion with a solids content of 2%, of which 70% by weight of the sodium salt of the phosphate diester of oleyl alcohol, which was reacted with 7 mol. of ethylene oxide, and 30% of an equimolar mixture of the bis-diethanolamine salt of monolauryl phosphate and of the diethanoiamine salt of dilauryl phosphate. · The treatment agent was passed by means of a rotating roller

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applied in such a tightness that 0.23% solids on the filaments, based on the weight of the filaments, were removed. The filaments were aged or lagged for 2.5 hours, at which time the maximum cold stretching 375% and they were able to get on with one. chlichen Streckzwirnma- machine without any difficulty at a ^ stretching degree or ratio of ^v 4>, 4-1-fold, and at a temperature of

hot-stretching pin to be stretched by 88 C /. Undrawn yarns produced as described above were retained or aged (approximately at 23 ° G) for a period of 1 day at room temperature, the maximum cold stretch being 368% and the yarns on a conventional draw-twisting machine at a draw ratio of 4, 67-f _a chen could be hot stretched without difficulty · This prepared in the manner vostehenden drawn yarns in.gekräuselte staple fibers were transferred and their elektrdjhschev'Eigenschaften on a Probenkarde or -krempel at .33% relative humidity and a temperature of 23 ° 0 checked »The cardboard or cardboard was equipped with an electrometer, an amplifier and an oacillograph in order to. Get a relative measure of the static electricity generated during the carding process · A linear system

encompasses (25 cm) the oscillograph track is - # a * wiekeHr or circled,

by a polar Pl is _a nimeter used which loading the

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ρ '

rich or the area in cm records, the previous experience under these test or test conditions has shown that

ρ
any »7th of 25 cm provides good static protection.

any value up to 4-0 cm is acceptable «The determination the static electricity of this staple fiber ^

5.5 cm,

Example 3

By means of extrusion or ejection from the melt of polyethylene terephthalate, which was modified with about 6; ό, based on the weight of polyethylene terephthalate, of methoxypolyethylene glycol with a molecular weight of about 2000 and about 0.125%, based on the weight of the polyethylene terephthalate, of pentaerythritol formed threads "the threads were then treated with an aqueous emulsion containing 10% solids of 100 percent _o -% contained the Fatriumsalzes of the phosphate diester of oleyl alcohol, which was reacted with 7 moles Äthylengocyd," the treatment agent was applied by a rotating roller in such a ^M close applied so that 0.70% solids to derrvFaden, based on the weight of the yarn, were deposited "". The thread yarns were then divided into 3 parts «. The first part was made directly on a customary stretch twisting machine. Hot stretched at a stretch of 4-, 4-1 with excellent results The second part was retained for 7 days, whereupon it was

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was hot-stretched with excellent results "The third part was retained long 31 days, whereupon the usmaß or on a common otreckzwirnmaschine at a draw _a draw ratio of 4.41-facheη was hot stretched with excellent Jrjjgebnisaen"

909804/1539

Claims (1)

Claims Ίο Procedure for granting a molecular orientation Filaments made from a polymeric polyester, characterized in that the filaments are impregnated with an aqueous emulsion, which is a phosphate ester surface treatment agent and an amine salt of an alkyl phosphate or mixtures of such Contains amine salts, and then the ports so impregnated stretched 2 · The method according to claim 1, 'characterized in that the solids content of the emulsion is about 70 to 100% by weight of a surface moisturizing agent and about. Contains 0 to 30% by weight of the amine salts 3o method according to claim 2, characterized in that the emulsion contains up to about 20% by weight solids * _4e Method according to one of Claims 1 to 3, characterized in that the threads are impregnated with an emulsion which contains about 2 to 15% by weight of solids, the surface treatment agent being composed of compounds of the general formula (7 -P-O OM ORIGINAL IMSPECTED 9O980A / 1239 ■ K69427 in which R is an alkyl radical having 8 "to 20 carbon atoms or an alkylphenyl radical in which the alkyl group has 8 to 20 carbon atoms, M is hydrogen, ammonium, an alkali metal or alkali metal and η is an integer from 2 to 20 inclusive, and compounds of general formula · _0M £ "Ή. - 0 - (CH ₂ GH ₂ O) _n JT '-P = 0 OM ^: in which R, M and η have the meaning given above, and the amine salt has the general formula 0
(RO) _x - P - ^ ~ 0 (HX) H7 _y has, in which χ a whole Z _R hl from 1 to 2, y difference between J and x, R a normal with 8 to 16 carbon atoms and HX an oxyalkyleneamine, which consists of an ethanolamine, H-methylethanolamine or morpholine, · 5> Method according to one of claims 1 to 4-, characterized in that that one threads made of a polyester from one with about 6%, based on the weight of the polyethylene terephthalate, of methoxy polyethylene glycol with a molecular weight from about 2000 and about 0.125 # »> based on the weight of the polyethylene terephthalate, modified by pentaerythritol Treated polyethylene terephthalate. BATH ORIGINAL 9098 (M / 1239 U69A27 - 50 - 6 ₀ A method according to, one of claims 1 "characterized to 5» in that one uses an emulsion whose solids content of 70 wt -..!. Yo of the sodium salt of the phosphate diester of reacted with 7 moles of ethylene oxide, oleyl alcohol and 30 % By weight of an equimolar mixture of the bisdiethanolamine salt of monolauryl phosphate and the -Ui & ethanolamine salt of dilauryl phosphate ". > 7. Method according to one of Claims 1 "to 5» characterized in that that an emulsion is used whose solids content from 100% by weight of the sodium salt of the phosphate diester of Oleyl alcohol, reacted with 7 moles of ethylene oxide, "consists of» 8 »Method according to one of claims Λ Ms 7», characterized in that the threads are impregnated with the aqueous emulsion in such a way that the solids mentioned in an amount of about 0.1 to 1.5% by weight, based on the Weight of the threads to be deposited » BATH ORIGINAL 909804/1239